Dioxoimidazolidine-3-acetate → 5-Hydroxy-1-(3-nitrobenzyl)-2,4-dioxoimidazolidine-3-acetic acid

HRID 1416398ノート

反応式

HRID 1416398 の反応式
[O:1]=C1CNC(=O)N1CC([O-])=O.[N+:12]([C:15]1[CH:16]=[C:17]([CH:31]=[CH:32][CH:33]=1)[CH2:18][N:19]1[C:23](=[O:24])[C:22](=[O:25])[N:21]([CH2:26][C:27]([OH:29])=[O:28])[C:20]1=S)([O-:14])=[O:13]>Cl.O1CCOCC1>[OH:24][CH:23]1[N:19]([CH2:18][C:17]2[CH:31]=[CH:32][CH:33]=[C:15]([N+:12]([O-:14])=[O:13])[CH:16]=2)[C:20](=[O:1])[N:21]([CH2:26][C:27]([OH:29])=[O:28])[C:22]1=[O:25]

参加物

5

反応物 2

HCID 2512551Dioxoimidazolidine-3-acetateHCID 106396263-(3-Nitrobenzyl)-4,5-dioxo-2-thioxoimidazolidine-1-acetic acid

生成物 1

HCID 108523655-Hydroxy-1-(3-nitrobenzyl)-2,4-dioxoimidazolidine-3-acetic acid

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

The above-prepared dioxoimidazolidine-3-acetate product of paragraph (2) (3.6 g) was dissolved in a mixed solvent of 4N hydrochloric acid and dioxane and the solution was stirred at room temperature for six hours. The reaction solution was concentrated in vacuo to dryness and then chloroform was added to the residue. The crystals were dislodged from the wall of the reaction flask with a spatula. The solid was collected by filtration, washed with chloroform and dried to give 0.8 g of 5-hydroxy-1-(3-nitrobenzyl)-2,4-dioxoimidazolidine-3-acetic acid [Compound 14] as amorphous crystals. The melting point, MS, IR, NMR, and elementary analysis for the compound were:

後処理

  1. concentrationThe reaction solution was concentrated in vacuo to dryness
  2. additionchloroform was added to the residue
  3. filtrationThe solid was collected by filtration
  4. washwashed with chloroform
  5. customdried

出典と根拠

ORDレコード
ord-d44e976853a54eb69ddafa30fea329b5
出典データセット
uspto-grants-1999_06
特許番号
US05912261

反応ノート

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